Textile wax compositions



,, terials.

Patented Dec. 14, 1948 TEXTILE WAX COMPOSITIONS George D. Jefferson,Kennett Square, Pa., as-

slgnor to Atlas Powder Company, Wilmington, Del., a corporation ofDelaware No Drawing. Application April 30, 1945,

Serial No. 591,237

The present invention relates to improvements in hydrocarbon waxcompositions.

' An object of the invention is to prepare a hydrocarbon wax compositionthat is particularly useful as a textile sizing material.

Another object is to provide such wax compositions that, afterthelrapplication, as for example as a textile size, are easily scourablein water.

A more specific object is to provide textile sizing compositions,certain of which are capable of application either in the form ofsolutions 'in hydrocarbon solvents or in the form of emulsions withwater, said compositions being capable of ready removal from the textilematerials by reason of their dispersibility in water.

The above and other objects will become more fully apparent in thecourse of the following description.

The invention will be described particularly with reference to its usein the textile art, but it will be understood that the composition hasproperties that are useful in other arts.

Hydrocarbon waxes represent a plentiful source of materials that possessphysical properties of lubricity and ability to form a coating, that aredesirable in the processing of textile ma- However, these waxes aresoluble only in certain non-aqueous solvents as a result of which theirusefulness in the textile field has been limited. Solutions ofhydrocarbon waxes can be applied to textile materials from non-aqueoussolvents, but they are particularly objectionable because of highsolvent retention and the difiiculty in removing all traces of the waxwhen that becomes necessary. In particular, it is desirable in theprocessing of certain textile materials to apply a waxy coating to ayarn for the purpose of retaining twistand imparting lubricity during aknitting operation. At the conclusion of the knitting operation, thewaxy coating must be removed to prepare the fabric for furtheroperations, such as dyeing, and to render the fabric suitable for use.The hydrocarbon waxes themselves have not been considered to be usefulas textile size materials because of the difficulties involved in theremoval of the hydrocarbon wax from the fabric without injury thereto.Various attempts have been made to mix hydrocarbon waxes with differentsubstances to render them more easily removable from a fabric. However,these earlier proposals have not been satisfactory either because of thecharacteristics of the compositions produced or because of the adverseeffects of the compositions on the textile material or the machines usedin handling it.

3 Claims. (Cl. 106--268) The present invention provides a hydrocarbonwax composition which has highly desirable coatterlals or on themachines used in handling them.

' polyoxyethylene ether ester of a straight-chain monobasic aliphaticacid having at least 12 car The compositions of the present inventioncomprise three ingredients; namely, the hydrocarbon wax, an emulsifierand a coupling or blending agent. The emulsifier has sufllcienthydrophylic properties to render the composition, which is otherwise ofa predominantly hydrophobe material, readily scourable in water. Thecoupling or blending agent tends to make the hydrophobe hydrocarbon waxand the hydrophilic emulsifier compatible, assists in making thecomposition scourable, and, at the same time,.

contributes other desirable properties to the composition. By varyingthe proportions of the materials, compositions of different degrees ofhardness, titer, etc. can be formulated for best results underparticular conditions.

The hydrocarbon 'wax employed in the compositions of the presentinvention is preferably a paraffin wax, for example, white crude scalewax of 124/126 A. M. P., a refined wax of /137 A. M. P. or a blnd ofparaffin wax with petrolatum or mineral 011. Other petroleum waxes, thefossil waxes or blended waxes such as'ceresin can be used. As will beunderstood, other types of waxes such as carnauba, beeswax, or Japanwax, can be blended with the hydrocarbon wax to alter the physicalproperties of the latter.

The emulsifier used in the wax composition of the invention is awater-dispersible to.soluble bon atoms and not more than one unsaturatedcarbon to carbon bond. As is well-known, the minimum number ofoxyethylene groups in the water-dispersible to soluble esters of thisclass varies depending upon the chain length of the acid and the numberof the acid groups present. The esters having the longer chain acidsrequire more oxyethylene groups to make them waterdispersible than dothe esters of the shorter chain acids. Similarly, esters with two ormore acid groups present require more oxyethylene groups to make themwater-dispersible than do the esters having only one acid group present.While groups is permissible.

an ester having oxyethyiene: groups present an amount in excess of thenumber required make the ester water-soluble may be employed.

the' preferred esters are those in which the ox?- ethylene groups arenot present in great excess over the number required to renderthe esterwater-soluble. A large excess of oxyethylene groups over the numberrequired to render the ester soluble contributes nothing to the ultimateI composition and may render it too hydrophilic;

Examples of ether esters falling within this class are thevwater-dispersible to soluble polyethylene glycol'esters of the fattyacids. These esters can be prepared either by esterifying a polyglycolor by reacting the fatty acid with ethylene oxide. Of this type, thepreferred emulsifiers are the polyethylene glycol monoesters of thefatty acids which contain a number 0! oxyethylene groups equal at leastto the value where c is the number of carbon atoms in the acid. Aparticularly valuable member of this group is a polyglycol monostearateproduced by the reaction of ethylene oxide and stearic acid in theproportion of 20 mols of ethylene oxide per mol of stearic acid. Anotheremulsifier of this group-is the polyglycol laurat-e with about 8oxyethylene groups per mol of lauric acid. Further examples of thepolyethylene glycol ester type are the polyglycol distearates whichcontain from 20 to 40 ethenoxy groups.

Another group of ether esters falling within this class are those inwhich the cxyethylene groups are coupled to the acid through polyhydriccompounds, preferably those having at least 3 hydroxyi groups and from 3to 6 carbon atoms, such as glucose or other sugar, hexitols, hexitans,hexides, glycerol, diglycerol, or the like. Specific examples of theseemulsifiers are the products produced by adding an average of 20ethenoxy groups to a sorbitan monoester of lauric or stearic acid.

A further type of emulsifier that can be used is prepared by firstreacting a polyhydric composition such as a hexitol or sugar withethylene oxide to form a polyhydroxy ethyl ether and then partiallyesterifying the ether with the selected acid. A specific example of suchan emulsifier is a disterate of glucose polyoxyethylene ether in whichthe ether has approximately six oxyethylene groups per mol of glucose.

All of these emulsifiers contain a plurality of oxyethylene groups,other groups, and at least one ester group. Accordingly, the termpolyoxyethylene ether ester" is used to include all oi I thesevariations. Mixtures of two or more emulsifiers of this class can beused. It should also be noted that commercial products of the typesdefined are actually mixtures due. to the facts that commercial fattyacids are usually mixtures of homologous acids, and also the process bywhich the polyoxyethylene ether esters are made give rise to a number ofproducts rather than a single compound. In particular, reactions withethylene oxide produce a series of compounds of diilerentpolyoxyethylene chain lengths which are designated in trade and in theliterature by a single name referring to. the average chain length.While the polyoxyethylene chains are generally uninterrupted, it will beapparent that the presence of other hydrophilic oxyalkylene For example,the ether esters can contain polyoxyalkylene chains comassasss posed ofalternate oxyethylene and oxymethylene groups such as the compoundsproduced by reacting 1,3-dioxolane with the aliphatic acid or an esterthereof.

The coupling or blending agent used in the composition of the inventionis selected from the on solution in hydrocarbon solvent, and ondispersion in water.

The aliphatic acid used as coupling agent serves several other usefulfunctions in the composition, Among these other functions are thereduction of solvent pickup, or conversely more rapid release ofsolvent, which results in achieving a strong, firm coating within ashort time after applica tion. In the coating the free acid also has theeifect of tempering the composition and reducing powdering. The couplingagent is selected with due regard to the physical characteristics of thehydrocarbon wax and the emulsifier so that the final product has thedesired physical properties. As in the case oi the emulsifiers, thecoupling agents include materials ranging from liquids to hard waxes sothat by selecting different members of the series the characteristics ofthe compositions can be varied.

The proportions of the three ingredients may be varied over relativelywide ranges within which it is possible to obtain compositions withvariations in hardness, titer, film strength, ease of dispersibility inwater and other properties.- It is also possible to obtain a largenumber of compositions of different ingredients which have essentiallythe same properties. However, in the compositions of the presentinvention, the emulsifiers and coupling agent are each used insubstantial proportions, the emulsifier being present in the waxcomposition in a proportion of at least 6% and the coupling agent beingpresent in a proportion of at least 10%. The hydrocarbon wax may varyfrom 20 to 75%, th balance of 100% being made up of the emulsifier andcoupling agent. The preferred compositions of the present inventioncontain at least 40% of the wax. Thus, for example, a preferredcomposition is one containing from 40 to 70% white crude scale wax124/126 A. M. P., 10 to 40% stearic acid and 6 to 30% of a. polyglycolmonostearate produced by the reaction of ethylene oxide .and stearicacid in the proportion of 20 mols of eth lene oxide per mol of stearicacid.

Examples positions was compatible in the molten condition,

although in some cases it was necessary that a small amount of water, onthe order of 1% or less be present. Where the addition of this smallamount of water was required, it was noted to t i have no adverseeffecton hydrocarbon solvent solubility or the other properties oi thecomposition. The compositions in the table were soluble to the extent ofat least 50% in Stoddards solvent at a temperature of 60 C. and thecompositions were insoluble or substantially less than 50% soluble inthat solvent at room temperature. Solubility at elevated temperature isimportant since the preferred method of applying these As an example ofthe application to yarn of a composition or the present invention in theform of a solution of the composition in a hydrocarbon solvent, thefollowing is given.

A 50% solution of the composition of Example 1 in Stoddard solvent atabout 60 C. is prepared and the yarn is soaked therein for to 20minutes. The yarn is then removed from the solution and placed in acentrifugal extractor to 'waxy sizes to yarns is to treat the yarns witha 10 remove excess solution. The soaking and exwarm solution which,oicourse, makes the solvent tracting operation should be performed toleave evaporate more readily-after the yarn leaves the about 8 to 10% ofthe composition on the yarn. bath. Insolubility at room temperatureiacili- Following the extraction, the yarn'can be wound tates completesolvent release from the coating. immediately on spools and then twistedor used The compositions were also evaluated for disin other ways.During a twistin operation, the persibility in water by stirring 10grams of the residual Stoddard solvent evaporates and the composition in200 cc. of distilled water at 60 waxy coating servesto hold the twist inthe yarn. C. The emulsions so prepared were allowed to Whether the yarnis twisted or not, the waxy stand overnight to determine theirstability. All coating is advantageous because of the lubricity of thecompositions in the table gave emulsions it imparts and the improvementin knitting and that remained stable by this test. handling propertiesresulting from its use. After Example Wax Percent oupling Agent PercentEmulsiiier Percent white crude scale 124/126 45 stearicacid .30polygly'col monostearatc average 20 ethenoxy 26 A. M. P. groups per molstearic acid.

50 so ..do

do palmitic acid ..do 76 ..do 20 myristic acid. 30 ..do 60 ...do... 20..do 60 stearic acid...

46 ..do 45 ..do

45 28 microcrystalline 30 20 white crude scale 124/126 50 A.M.P. 30 doSi -do The compositions are prepared as indicated above by mixing theingredients together at a temperature suiflcient to melt them all. Aftercooling, the product is preferably comminuted or powdered for theconvenience of users.

The compositions of the present invention'may be applied to yarn orother products which it is yarns such as yarns of viscose rayon,cuproammonium rayon and cellulose acetate. The compositions can beapplied to yarn in skein or cake form or on 53 or twister bobbins.

position from the material. v

lose acetate knitted goods are completely scoured polyglycol distearate,average 20 ethenoxy groups perm v sorbitan trioieate polyglycol ether,20 ethenoxy groups.

sorbitan monostearate poiyglycol ether, 20 ethonox groups.

pol g yool distearate, 40 ethenoxy groups sor itnntrioleate polyglycolether, 20 othenoxy oups.

po yzlycol monostearate, 20 othenoxy groups distearate oi glucosepolyoxycthylene other, 6

ethenoxy groups.

sorbitan monolaurate polyoxyethylene ether, 20

ethcnoxy groups.

sorbitan monostearate polyoxyethylone ether, 20

ethenoxy groups per mol.

8 8 888! i E3 53 88888588$23888f2858 Q the yarn is knitted, for example,the waxy composition can be removed either in a. separate operation orin the dye bath. In a combined scouring and dyeing operation in the caseof knitted viscose it is recommended to use a boiling solution of thedyes, 6% soap, 2% pine oil, and 3% tetrasodium pyrophosphate based onweight of the goods. ,After 10 minutes of scouring and dyeing Glauberssalt is added in amounts up to 5%. The goods are then removed from thebath, rinsed, and finished for use. It is not necessary to use a boilingsolution to scour the waxy com- For example, celluand dyed in a bath ata temperature of about 160 F. (71 C.)

The following is an example of the application of a composition of theinvention to yarn by means of an aqueous emulsion. An emulsioncontaining 10 to 20% of the composition of Example 1 is prepared bymixing the composition and water at about 60 C. The yarn is then soakedin the emulsion, extracted in a centrifuge,

and dried. The yarn then carries the waxy coating and can be usedln thesame way as the yarn treated with hydrocarbon solution described above.An advantage of the composition used resides inthe fact that evendistribution is obtained when yarn in cake form is soaked in theemulsion. ,A number of emulsiilable compositions that have beensuggested as yarn sizes give unsatisfactory results on application toyarn in this form due to a wicking eifect which concentrates the size atthe outside layer of the cake.

In the foregoing examples of yarn sizing, the treating baths.hydrocarbon solvent solutions or 40 to 70% paramn scale wax, 6 to 30% ofa polyaqueous emulsions can be used repeatedly with necessaryreplacement or the-amount absorbed by the yarn. Likewise the eiiluentfrom the centrifugal extractor can be returned to the bath and reused.

The invention has been described as applied to use as a textile sizesince it is in that field that it has the greatest usefulness at thepresent time. The properties of the compositions of the invention,however. suggest their use for other purposes where it is advantageousto deposit a waterdispersible waxy coating on a surface.

It will be understood that the compositions oi the invention can be usedin conjunction with other substances. Various substances, such as.coloring agents or agents designed to accomplish some other effect onthe yarn or other material to be treated, can be added to thecompositions or to their solutions or emulsions provided, of course.that they do not adversely affect the composition.

What is claimed is:

ethylene glycol monostearate produced 'by the reaction of ethylene oxideand stearic acid in the proportion of about 20 mols ethylene oxide permol of stearic acid, and 10 to 40% stearic acid, to

make a total of 100% of said mixture.

3. A solid composition consisting essentially of about paraflln scalewax of 124/126 A. M. P., about 30% stearic acid, and about 25% of apolyethylene glycol monostearate produced by the reaction oi ethyleneoxide and stearic acid in the proportion of 20 mols ethylene oxide permol of stearic acid.

GEORGE D. JEFFERBON.

REFERENCES CITED The following references are of record in the file ofthis patent:

UNITED s'm'ms PA'I'ENTS

